US11975276B2 - Process monitoring and control of filtration by means of filtrate measurements - Google Patents
Process monitoring and control of filtration by means of filtrate measurements Download PDFInfo
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- US11975276B2 US11975276B2 US17/047,643 US201917047643A US11975276B2 US 11975276 B2 US11975276 B2 US 11975276B2 US 201917047643 A US201917047643 A US 201917047643A US 11975276 B2 US11975276 B2 US 11975276B2
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- 238000001914 filtration Methods 0.000 title claims abstract description 75
- 239000000706 filtrate Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000012544 monitoring process Methods 0.000 title claims abstract description 14
- 238000005259 measurement Methods 0.000 title claims description 81
- 238000005406 washing Methods 0.000 claims abstract description 69
- 238000004458 analytical method Methods 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 239000013590 bulk material Substances 0.000 claims abstract description 7
- 238000011156 evaluation Methods 0.000 claims description 14
- 230000001186 cumulative effect Effects 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 60
- 239000012065 filter cake Substances 0.000 description 58
- 239000002609 medium Substances 0.000 description 37
- 239000011780 sodium chloride Substances 0.000 description 30
- 239000007787 solid Substances 0.000 description 19
- 239000012452 mother liquor Substances 0.000 description 15
- 238000002474 experimental method Methods 0.000 description 11
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
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- QOIYTRGFOFZNKF-UHFFFAOYSA-N flupyradifurone Chemical compound C=1C(=O)OCC=1N(CC(F)F)CC1=CC=C(Cl)N=C1 QOIYTRGFOFZNKF-UHFFFAOYSA-N 0.000 description 3
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
- B01D9/0045—Washing of crystals, e.g. in wash columns
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/60—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor integrally combined with devices for controlling the filtration
- B01D29/601—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor integrally combined with devices for controlling the filtration by clearness or turbidity measuring
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/085—Funnel filters; Holders therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
Definitions
- the application relates to solutions for the monitoring, process control and supervision of a solids filtration, especially of the operation of washing these solids, in a filtration plant.
- the solids are a free-flowing material, typically the result of a crystallization or precipitation in the form of granules or powder, and generally also referred to as solid-state bulk material.
- Customary production process for production of solid active ingredients from crystallization or precipitation onwards is subdivided as follows:
- Customary filter apparatuses are, for example, suction filters, centrifuges, drum or disk filters etc., but also porcelain or glass funnels with flat sieving surfaces or frits, or another porous filter element.
- a suction filter for example, the suspension to be filtered is transferred to the apparatus, the filtrate is separated from the solids under pressure or vacuum, and led off.
- a suction filter is shown in schematic form by way of example in FIG. 1 .
- step 3 of a solids filtration the filtercake is subsequently washed in a displacement and/or resuspension washing operation in order to “wash the solids clean”, i.e. to attain the quality features required for the solids.
- fixed amounts of solvent fresh or recycled
- the number of washes is dependent on the required purity of the solids.
- the filter apparatus is not opened between the wash steps, and so sampling of the filtercake is not possible for that and other reasons.
- step 4 This is typically accomplished either on the pressure suction filter (suction drier) as well or in a separate drying step.
- steps 3 and 4 there may also be formulation steps, for example addition of plasticizers, stabilizers etc.
- the filtration and washing operation is regarded as a “black box” which is optimized by trial and error (Ruslim et al., Chemical Engineering Science 62 (2007) 3951-3961). Ruslim et al. addresses the problem of heterogeneous distribution of the wash media in a filtration and washing operation. He studies a measurement of the filtercake online, but prefers offline measurement, and writes that measurements of the filtercake are better, rather than measurement of the filtrate stream. He uses the measurement of the filtrate stream merely for complete examination for impurities.
- LOUHI-KULTANEN et al. describes a method and a measurement apparatus for control of a filtration and washing operation with a Raman spectrometer in which a measurement is likewise conducted in the filtercake. This is a local measurement (on the cake surface) or an invasive measurement method (immersion optics) that damages the filtercake. Furthermore, this method does not enable trace measurements since the measurement limit of a Raman spectrometer is 1%. LOUHI-KULTANEN et al.
- step 4 quality control of the solids while they are still in the filter apparatus (i.e. point 2 or 3) does not take place in industrial filtration and washing operation processes.
- the analysis is conducted merely after conclusion of step 4.
- solid samples are taken from the dried filtercake and analyzed in the laboratory, usually by means of chromatography. It is generally assumed in the specialist field that the quality of the filtercake can be ascertained only by direct filtercake analysis. As a result, the monitoring of the quality of filtercakes in the filtration process has been unaffected to date by the advances of online measurement technology. If the filtercake tested does not meet the specification, the dried product therefore has to be reprocessed, discarded or cut.
- the amount of wash medium and the wash strategy (displacement, countercurrent or slurry wash) is typically ascertained experimentally once and validated by analysis of the filtercake.
- Kopra et al. discloses a process and a measurement apparatus for control of the filtration and washing operation for the paper industry in a pulp wash with a refractometer.
- the refractive index of the wash medium which is guided into the filter apparatus and out of the filter apparatus is determined, with the aim of ascertaining whether the wash medium can be reused.
- the wash medium feed is adjusted using the measurements in order to avoid unwanted wash losses.
- Kopra et al. does not give any pointer as to the utilization of these measurements in order to obtain conclusions as to the progression of the washing operation or the quality of the filtercake. In view of the filter apparatus, this would not be possible in any case since there is no separate measurement from the respective wash zones. (Kopra et al.
- the object was achieved by the use of measurement technology for measurement in the filtrate stream from a filter apparatus, wherein parameter values of the filtrate stream are measured over the period of the filtration and washing operation, and the changes in these are analyzed over the period of time. It has been found that, surprisingly, this analysis during the filtration enables conclusions as to the progress and quality of the filtration and washing process.
- the application firstly provides a method of monitoring and of controlling a filtration and washing operation of a solid-state bulk material in a filter apparatus for cake filtration according to claim 1 and the claims dependent thereon, wherein at least one measurement apparatus is mounted in or on the filtrate outlet of the filter apparatus, which measures one or more parameters of a filtrate stream from the filter apparatus for cake filtration during the washing operation, and the change in the parameter values measured is analyzed over the period of time.
- Suitable measurable parameters of the filtrate stream in the context of the application are especially refractive index, density, ultrasound transit time, redox potential and spectroscopic cumulative and/or substance-specific properties of at least one representative constituent in the filtrate stream (main and/or secondary component), for instance absorption, impedance, color or the fluorescence signal of the filtrate.
- main and/or secondary component for instance absorption, impedance, color or the fluorescence signal of the filtrate.
- pH and/or conductivity it is also possible to use pH and/or conductivity.
- the selection of the measurement method depends on the substances used in the process (especially product(s) and/or byproduct(s)). Particular preference is given to using the measurement of the refractive index and/or the density of the filtrate over the course of the filtration and wash. It is also possible to combine one or more of the abovementioned methods. It is likewise possible, for quality control, as well as the pure measurement values (raw data), also to ascertain concentrations of the (secondary) components using calibration functions ascertained beforehand.
- a parallel recording of refractive index and the measurement of the filtrate mass customary in the art are conducted.
- the method is suitable both for the monitoring of a continuous process and for the monitoring of a batchwise process.
- wash medium is metered continuously onto the filtercake, such that the filtercake is covered homogeneously over its entire area.
- a predefined amount of wash media is applied to the filtercake for the wash.
- the method comprises computer-implemented steps for analysis of the measurement data.
- these steps are performed by an appropriately configured computer system.
- the measurement apparatus(es) For the analysis of the measurement data, these are transmitted from the measurement apparatus(es), for example via a data interface (OPC, SQL, fieldbus, e.g. profibus, modbus, Ethernet, analog signal etc.); the imported measurement data are stored in an archiving module, for example a database module in which the measurement data and a timestamp t and preferably all information for clear identification of the production batch are recorded.
- OPC data interface
- SQL e.g. profibus, modbus, Ethernet, analog signal etc.
- an archiving module for example a database module in which the measurement data and a timestamp t and preferably all information for clear identification of the production batch are recorded.
- the database module is connected to an evaluation system.
- An evaluation system in the context of the application is a measurement control system or a computer configured for the performance of the method steps.
- the application therefore further provides a computer system for control of a filtration and washing operation on a solid-state bulk material in a filter apparatus for cake filtration, wherein the computer system comprises:
- the evaluation system is connected to a system for control of a wash medium feed and configured to be able to issue commands for continuation or ending of the wash medium feed.
- the feed of the wash medium is started and ended with the aid of the evaluation system, or a new washing operation is occasioned by virtue of the evaluation system issuing the corresponding command to a controllable wash medium feed (e.g. valves).
- a controllable wash medium feed e.g. valves
- the wash medium feed is controllable via one or more control elements for control of the wash medium feed (e.g. a process control system).
- a limit value assessment and/or change analysis is conducted.
- the measurement data analysis in a limit value assessment of the raw data or of the concentration values calculated therefrom, typically comprises the following steps:
- the wash strategy is altered; it is possible, for example, to conduct a slurry wash (suspension wash) or a combination of displacement and slurry washes.
- the method comprises steps for change analysis of the raw data or of the concentration values ascertained from the raw data.
- the measurement data analysis in a change analysis of the raw data or of the concentration values calculated therefrom, typically comprises the following steps:
- the quality of the wash is ascertained from the measurement data by means of one or more further data analyses.
- the slope of the measurement curve (between two measurements, for example between measurements of the timestamp t ⁇ 1 and t) is preferably calculated in period C.
- the calculated slope is compared with a range of values (working range) for the slope that has been predefined as being approved; this has typically been ascertained from prior washes with satisfactory quality.
- the system issues a warning; the system optionally ends the washing operation.
- the effectiveness of the washing operation is ascertained by the following steps:
- the optimal wash ratio is determined from the analysis of the wash curve (measurement via wash ratio FIG. 3 or 5 ) for the subsequent batches. If there is no further change in the measurement, the optimal wash ratio, i.e. the optimal amount of wash medium, has been exceeded.
- the amount of wash medium consumed for the washing operation until the calculated end of the washing operation is ascertained and fixed as the optimal amount of wash medium for the next washing operation.
- the new amount of wash medium for washing of the filtercake is added.
- the amount of wash medium is calculated online and a warning is given, for example, in the event of exceedance of the optimal amount of wash medium.
- the measurements may be considered/interpreted either online or subsequently in their entirety (process optimization).
- the measurement in the filtrate stream from a filter apparatus for cake filtration and the subsequent analysis of the measurements obtained can achieve a product-specific validation of the quality of the filtercake in association with the concentration of the secondary components in the filtrate stream or with the measurable cumulative parameter of the filtrate stream.
- the method provides the following information as to the progression of the process:
- the determination of refractive index is used as cumulative signal with respect to the secondary components.
- a measuring instrument positioned correspondingly in the filter apparatus is used to determine the measurement online, for example the refractive index in the filtrate stream.
- the measuring instrument is preferably installed in the filtrate outlet 5 —either in an unpressurized manner or optionally in a pressure conduit ( FIG. 1 ).
- the measurement and its variation over time can be used as a feature for quality control.
- the value measured online is compared with a calibration function ascertained beforehand between measurement and secondary components/product quality ( FIG. 2 ).
- the application further provides a filter apparatus comprising a wash medium feed, a filter element, a filtrate outlet and a measurement apparatus for measurement in the filtrate stream, wherein the measurement apparatus is selected for measurement of one or more parameters, for example refractive index, density, ultrasound transit time, pH, conductivity, redox potential and/or spectroscopic properties of the filtrate stream.
- the measurement apparatus is installed in or on the filtrate outlet.
- the measurement apparatus is installed into the filtrate conduit of the filter apparatus.
- the filter apparatus additionally comprises a measurement apparatus for measuring the mass of filtrate.
- a measurement apparatus for measuring the mass of filtrate.
- the mass of filtrate in the filtrate collection vessel is ascertained/recorded.
- the mass of filtrate is ascertained/recorded with the aid of a flowmeter from the volume flow rate/mass flow rate.
- the measurement is combined with a measurement of the mass of filtrate.
- Suitable filter apparatus are suction filters, centrifuges, Büchner funnels, frits, filter crucibles, drum filter, disk filter, belt filter and filter press, without being limited thereto.
- the refractive index is suitable as a cumulative signal for detecting decrease in concentration in the filtrate; variances from the expected value in the concentration and the filtration rate per unit time can be shown and recognized.
- a process refractometer was integrated into the filtrate outlet of the laboratory test bed for filtration as the online measurement technique.
- a process refractometer of the PR-43 type from KPatents having a measurement range of nD 1.32-1.53 was used.
- a flow adapter was used for the laboratory experiments.
- the filtration and wash experiments were conducted in a 100 cm 2 laboratory pressure filter at 0.2 bar gauge and room temperature.
- the process refractometer (Abbemat300 from Anton) was integrated in the filtrate conduit. Refractive index and mass of filtrate were recorded in a time-resolved manner. After the end of the experiment, the height and mass of the filtercake were determined.
- the refractive index of the mother liquor filtrate and of the wash filtrate was determined with an Abbemat 300 from Anton Paar at 23° C.
- Model particles used were SiLibeads type S 0-50 ⁇ m glass beads (sourced from Sigmund Lindner GmbH). The solids concentration was 400 g/kg. The impurity used was NaCl in a concentration of 200 g/kg. The amount of suspension applied was about 1000 g, i.e. 120 g of NaCl was introduced into the system as a dissolved impurity. For the wash, 1192 g of ultrapure water was used (corresponding to a wash ratio 4.3 l of water/l of dry filtercake), in order to obtain a very clean filtercake.
- FIG. 5 shows the progression of the refractive index (RI) against the wash ratio. It is clearly apparent that the constant measurement of the mother liquor filtrate is lowered by the increasing amount of water. At the end of the wash, a plateau value is attained.
- Quantitative evaluation can be effected with a higher degree of complexity for real products. For the model project, this is set out hereinafter.
- the plot of the RI and of the mass of filtrate against time for filtration and wash is chosen (see FIG. 5 ).
- the mass of filtrate and mass of NaCl can be calculated from the data recorded via an NaCl concentration-refractive index calibration line.
- m NaCl,1 ( m filtrate,1 ⁇ m filtrate,0 )* c NaCl,1
- integration of the curve can also be performed as follows:
- the masses of filtrate and refractive indices in the filtrates collected were determined. This can be used to calculate a mass balance.
- 120 g of NaCl were used in the experiment detailed.
- 414 g of mother liquor filtrate with a concentration of 200 g/kg NaCl and 1347 g of wash filtrate with a concentration of 24 g/kg NaCl were collected.
- the result is 83 g of NaCl dissolved in the mother liquor filtrate and 32 g of NaCl dissolved in the wash filtrate. Since no NaCl was detectable in the filtercake, it was possible to recover 115 g of NaCl in the filtrates by measurement technology.
- the refractive index decreases during the wash from the (starting) value of the mother liquor to a lower (plateau) value at the end of the wash.
- the curve thus falls with a particular slope. If there is any change in this slope, it is possible to conclude the quality of the wash therefrom.
- FIG. 6 A shows the progression and in particular the increase in the refractive index. This suggests that the wash front does not run homogeneously through the filtercake, but that discontinuities—channels here—have formed. This would not be apparent solely from visual inspection of the filtercake after the wash, as apparent in FIG. 6 B . In an inspection of the filtercake from above, as is technically possible, it is not possible to see any cracks, channels, etc. that are hidden within the filtercake.
- FIG. 1 Schematic diagram of a pressure suction filter
- FIG. 2 Representation of trend of the measured value (RI) against time, divided into process phases:
- A dislacement of the mother liquor
- B intermediate region
- C approved region
- D disiffusion region
- E end of the wash effect.
- FIG. 3 Comparison of refractive index ( ⁇ ) and sum total of the secondary components ( ⁇ ) for the product Sivanto.
- the refractive index of pure butanol at 20° C. is 1.39932. (Example A).
- FIG. 4 Mass of filtrate M ( ⁇ ) and refractive index RI ( ⁇ ) as a function of time t. Region 1: filtration; region 2: wash.
- FIG. 5 NaCl concentration ( ⁇ ) and refractive index RI ( ⁇ ) as a function of the wash ratio.
- FIG. 6 A Filtercake with channels, removal of moisture after mother liquor filtration.
- FIG. 6 B Filtercake after mechanical removal of moisture after wash.
- FIG. 7 ⁇ mass (M) and ⁇ refractive index (RI) as a function of time (t).
- FIG. 8 Block diagram of the method for control of the washing operation
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- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Detergent Compositions (AREA)
Abstract
Description
-
- 1. Crystallization/precipitation, also called solids formation: This step of the production process forms the solids suspended in mother liquor,
- 2. Filtration: the solids are separated from the mother liquor in a filtration apparatus for pressure, vacuum or centrifugal filtration (also referred to collectively as filter apparatuses hereinafter).
-
- an archiving module configured for the storage of parameter values of a filtrate stream with a timestamp t transmitted from at least one measurement apparatus in or on the filtrate outlet of the filter apparatus over the period of the filtration and washing operation and for the transfer of these to an evaluation system,
- the evaluation system connected to the archiving module and configured to analyze changes in the parameter values over the period of time, and to use this change analysis to ascertain the end of the filtration and washing operation and/or the effectiveness of the washing operation,
- a display element for the end of the filtration and washing operation and/or the effectiveness of the washing operation, and/or
- an element for issuing a command to end the filtration and washing operation.
-
- 1. Transfer of the measurements of the monitored parameters of the filtrate stream to the evaluation system over a predefined period of time in the filtration and wash process at least until attainment of a predefined parameter value that has been ascertained experimentally beforehand or from experience and corresponds to the desired quality of the filtercake. If this value is attained, it can be assumed that the filtercake has been washed in accordance with the specification; the washing operation can be ended.
- 1.1. In a continuous process, on attainment of the parameter value from 1, the feed of the wash medium is ended; the filtercake is processed further.
- 1.2. In a batchwise process, the end of the wash process is communicated. For the next batch wash of a further filtercake, it is optionally possible to adjust (typically reduce) the amount of wash medium in accordance with the predefined parameter from 1. The method of adjusting the amount of wash medium is described in detail further down.
- 2. If the predefined parameter value (see 1.) is not attained, it can be assumed that the filtercake has not been washed optimally; the wash operation is continued by
- 2.1. In a continuous process, the wash medium feed is extended.
- 2.2. In a batchwise process, an additional wash may follow for the already washed cake. In the next batch with a new filtercake, the amount of wash medium can be increased.
- 1. Transfer of the measurements of the monitored parameters of the filtrate stream to the evaluation system over a predefined period of time in the filtration and wash process at least until attainment of a predefined parameter value that has been ascertained experimentally beforehand or from experience and corresponds to the desired quality of the filtercake. If this value is attained, it can be assumed that the filtercake has been washed in accordance with the specification; the washing operation can be ended.
-
- 3. Transfer of the measurements of the monitored parameters of the filtrate stream into the evaluation system over a predefined period of time in the filtration and washing process. Calculation of the first derivative of a curve generated from the measurements. If the first derivative (=slope) of the measurement curve ceases to change or is below a predefined value, the following measures may be taken:
- 3.1. In a continuous process, the feed of the wash medium is ended. In accordance with the limit value assessment from 1. (attained/not attained), further measures are optionally taken, for example a change in the wash strategy.
- 3.2. In a batchwise process, the end of the wash process is communicated. For the next wash step, the amount of wash medium is optionally adjusted (reduced or increased) in accordance with the limit value assessment from 1.
- 3. Transfer of the measurements of the monitored parameters of the filtrate stream into the evaluation system over a predefined period of time in the filtration and washing process. Calculation of the first derivative of a curve generated from the measurements. If the first derivative (=slope) of the measurement curve ceases to change or is below a predefined value, the following measures may be taken:
-
- a) The slope is too flat, caused, for example, by cracks in the filtercake.
- b) The slope is nonuniform, caused, for example, by holes or channels in the filtercake.
The assessment of the slope enables understanding or monitoring of the process, such that suitable countermeasures can be initiated. These may be, for example: noting the (under)saturation of the filtercake, checking the filter medium used for faults, smoothing the filtercake etc.
-
- a) An elevated slope means an elevated washing speed, which can be achieved, for example, by an elevated pressure. This results in a shorter wash time, which reduces the cycle time.
- b) A reduced slope means an increased wash time. This increases the diffusion time of the wash medium into the solid-state pore system, which can increase the wash effectiveness.
-
- Effectiveness of the wash
-
- a) a period C in which the measurement curve changes with a slope of at least or equal to a predefined value X is ascertained from the measurement curve (see
FIG. 2 ), - b) a slope value is calculated as the average slope over the period C from a),
- c) a variability of the slope in section C from a) is calculated,
- d) if the slope value is within the predefined working range and the variability of the slope is less than X, washing operation is running effectively; the washing operation is continued until the slope value attains a predefined value for a sufficient wash quality,
- e) if the slope value is ≤a predefined minimum value (flat slope) and/or the variability of the slope value is high, there is a suspicion of gradient formation or discontinuity in the cake. A warning is issued and/or filtration pressure is increased.
- a) a period C in which the measurement curve changes with a slope of at least or equal to a predefined value X is ascertained from the measurement curve (see
-
- assessment of the progress of the process,
- identifying a stoppage/endpoint criterion
- identifying process faults, for example irregular filtercake structure
- Stability of the process
- Pointers for optimization of the amount of wash medium
This information is used to conduct an indirect filtercake analysis.
-
- ii.
- iii. Experimental Evaluation:
-
- The mass of filtrate increases during the filtration and wash, before remaining constant during the removal of moisture from the filtercake at the end of the experiment. The refractive index remains constant during the filtration since only mother liquor leaves the filtercake. In the subsequent wash, the refractive index decreases from the value of the mother liquor to the value of the pure wash medium.
m NaCl,1=(m filtrate,1 −m filtrate,0)*c NaCl,1
Area in period of time: A 1=0.5*(t 1 −t 0)*(c NaCl,1 −c NaCl,0)
By reference to the time interval and the mass of filtrate recorded in this time interval, it is possible to determine the mass of NaCl in the time interval (see tables 1 and 2).
TABLE 1 |
Integration of the measurement data for filtration |
Time | Delta t | Mass | Delta m | NaCl | Individual area | Individual area | Mass of NaCl | |
s | s | RI | g | g | g/kg | s * g/kg | g/kg | g |
0.00 | 1.00 | 1.36823 | 12.4 | 12.4 | 200.2 | 197.7 | 197.7 | 2.46 |
1.00 | 1.00 | 1.36821 | 25.8 | 13.4 | 200.1 | 200.2 | 200.2 | 2.68 |
2.00 | 1.00 | 1.36824 | 41.2 | 15.4 | 200.3 | 200.2 | 200.2 | 3.08 |
3.00 | 1.00 | 1.36816 | 53.0 | 11.8 | 199.8 | 200.1 | 200.1 | 2.36 |
4.00 | 1.00 | 1.36813 | 66.1 | 13.1 | 199.7 | 199.7 | 199.7 | 2.62 |
5.00 | 1.00 | 1.36816 | 80.1 | 14.0 | 199.8 | 199.7 | 199.7 | 2.79 |
6.00 | 1.00 | 1.36812 | 90.8 | 10.7 | 199.6 | 199.7 | 199.7 | 2.14 |
7.00 | 1.00 | 1.36811 | 103.1 | 12.3 | 199.5 | 199.6 | 199.6 | 2.45 |
8.00 | 1.00 | 1.3681 | 115.8 | 12.7 | 199.5 | 199.5 | 199.5 | 2.54 |
9.00 | 1.00 | 1.36811 | 126.1 | 10.4 | 199.5 | 199.5 | 199.5 | 2.07 |
10.00 | 1.00 | 1.36812 | 134.6 | 8.5 | 199.6 | 199.6 | 199.6 | 1.69 |
11.00 | 1.00 | 1.36808 | 144.1 | 9.4 | 199.4 | 199.5 | 199.5 | 1.88 |
12.00 | 1.00 | 1.36806 | 152.9 | 8.8 | 199.3 | 199.3 | 199.3 | 1.76 |
13.00 | 1.00 | 1.36808 | 166.6 | 13.7 | 199.4 | 199.3 | 199.3 | 2.73 |
14.00 | 1.00 | 1.36805 | 176.0 | 9.5 | 199.2 | 199.3 | 199.3 | 1.89 |
15.00 | 1.00 | 1.36811 | 186.0 | 10.0 | 199.5 | 199.4 | 199.4 | 1.99 |
16.00 | 1.00 | 1.3681 | 194.8 | 8.7 | 199.5 | 199.5 | 199.5 | 1.74 |
17.00 | 1.00 | 1.36808 | 202.7 | 7.9 | 199.4 | 199.4 | 199.4 | 1.57 |
18.00 | 1.00 | 1.36803 | 211.1 | 8.4 | 199.1 | 199.2 | 199.2 | 1.68 |
19.00 | 1.00 | 1.36803 | 220.1 | 9.0 | 199.1 | 199.1 | 199.1 | 1.79 |
20.00 | 1.00 | 1.36802 | 228.3 | 8.2 | 199.0 | 199.1 | 199.1 | 1.63 |
21.00 | 1.00 | 1.36803 | 236.6 | 8.3 | 199.1 | 199.1 | 199.1 | 1.65 |
22.00 | 1.00 | 1.36804 | 243.7 | 7.2 | 199.2 | 199.1 | 199.1 | 1.43 |
23.00 | 1.00 | 1.36803 | 252.4 | 8.7 | 199.1 | 199.1 | 199.1 | 1.73 |
24.00 | 1.00 | 1.36803 | 258.0 | 5.6 | 199.1 | 199.1 | 199.1 | 1.12 |
25.00 | 1.00 | 1.36803 | 266.9 | 8.9 | 199.1 | 199.1 | 199.1 | 1.78 |
26.00 | 1.00 | 1.36803 | 273.8 | 6.9 | 199.1 | 199.1 | 199.1 | 1.37 |
27.00 | 1.00 | 1.36802 | 280.8 | 7.0 | 199.0 | 199.1 | 199.1 | 1.40 |
28.00 | 1.00 | 1.36803 | 289.3 | 8.5 | 199.1 | 199.1 | 199.1 | 1.70 |
29.00 | 1.00 | 1.36803 | 297.8 | 8.5 | 199.1 | 199.1 | 199.1 | 1.69 |
30.00 | 1.00 | 1.36803 | 305.2 | 7.4 | 199.1 | 199.1 | 199.1 | 1.47 |
31.00 | 1.00 | 1.36802 | 313.2 | 8.0 | 199.0 | 199.1 | 199.1 | 1.58 |
32.00 | 1.00 | 1.368 | 320.6 | 7.4 | 198.9 | 199.0 | 199.0 | 1.47 |
33.00 | 1.00 | 1.36797 | 328.4 | 7.9 | 198.8 | 198.8 | 198.8 | 1.56 |
34.00 | 1.00 | 1.368 | 335.3 | 6.8 | 198.9 | 198.8 | 198.8 | 1.36 |
35.00 | 1.00 | 1.36797 | 342.6 | 7.3 | 198.8 | 198.8 | 198.8 | 1.45 |
36.00 | 1.00 | 1.36803 | 350.1 | 7.5 | 199.1 | 198.9 | 198.9 | 1.49 |
37.00 | 1.00 | 1.36803 | 357.3 | 7.3 | 199.1 | 199.1 | 199.1 | 1.44 |
38.00 | 1.00 | 1.368 | 365.2 | 7.8 | 198.9 | 199.0 | 199.0 | 1.56 |
39.00 | 1.00 | 1.36795 | 373.2 | 8.0 | 198.6 | 198.8 | 198.8 | 1.59 |
40.00 | 1.00 | 1.36798 | 380.3 | 7.2 | 198.8 | 198.7 | 198.7 | 1.43 |
41.00 | 1.00 | 1.368 | 387.4 | 7.1 | 198.9 | 198.9 | 198.9 | 1.41 |
42.00 | 1.00 | 1.36797 | 393.4 | 5.9 | 198.8 | 198.8 | 198.8 | 1.18 |
43.00 | 1.00 | 1.36803 | 400.8 | 7.4 | 199.1 | 198.9 | 198.9 | 1.47 |
44.00 | 1.00 | 1.368 | 409.0 | 8.2 | 198.9 | 199.0 | 199.0 | 1.63 |
45.00 | 1.00 | 1.36794 | 411.4 | 2.4 | 198.6 | 198.8 | 198.8 | 0.48 |
46.00 | 1.00 | 1.36794 | 412.8 | 1.4 | 198.6 | 198.6 | 198.6 | 0.27 |
47.00 | 1.00 | 1.36794 | 413.4 | 0.6 | 198.6 | 198.6 | 198.6 | 0.13 |
48.00 | 1.00 | 1.36794 | 413.7 | 0.3 | 198.6 | 198.6 | 198.6 | 0.06 |
49.00 | 1.00 | 1.36794 | 414.0 | 0.3 | 198.6 | 198.6 | 198.6 | 0.06 |
50.00 | 1.00 | 1.36792 | 414.2 | 0.2 | 198.5 | 198.5 | 198.5 | 0.04 |
51.00 | 1.00 | 1.3679 | 414.2 | 0.0 | 198.4 | 198.4 | 198.4 | 0.00 |
52.00 | 1.00 | 1.36794 | 414.2 | 0.0 | 198.6 | 198.5 | 198.5 | 0.00 |
Total NaCl filtration: 83 g |
TABLE 2 |
Integration of the measurement data for wash |
Time | Delta t | Mass | Delta m | NaCl | Individual area | Individual area | Mass of NaCl | |
s | s | RI | g | g | g/kg | s * g/kg | g/kg | g |
172.00 | 1.00 | 1.36804 | 0.0 | 0.0 | 199.2 | 199.3 | 199.3 | 0.00 |
173.00 | 1.00 | 1.36805 | 0.0 | 0.0 | 199.2 | 199.2 | 199.2 | 0.00 |
174.00 | 1.00 | 1.36811 | 1.1 | 1.1 | 199.5 | 199.4 | 199.4 | 0.22 |
175.00 | 1.00 | 1.36811 | 5.7 | 4.6 | 199.5 | 199.5 | 199.5 | 0.91 |
176.00 | 1.00 | 1.36811 | 13.5 | 7.8 | 199.5 | 199.5 | 199.5 | 1.56 |
177.00 | 1.00 | 1.36813 | 19.9 | 6.4 | 199.7 | 199.6 | 199.6 | 1.27 |
178.00 | 1.00 | 1.36817 | 26.0 | 6.1 | 199.9 | 199.8 | 199.8 | 1.21 |
179.00 | 1.00 | 1.36812 | 33.1 | 7.2 | 199.6 | 199.7 | 199.7 | 1.43 |
180.00 | 1.00 | 1.36811 | 38.2 | 5.0 | 199.5 | 199.6 | 199.6 | 1.00 |
181.00 | 1.00 | 1.36811 | 46.7 | 8.5 | 199.5 | 199.5 | 199.5 | 1.70 |
182.00 | 1.00 | 1.36811 | 52.9 | 6.2 | 199.5 | 199.5 | 199.5 | 1.24 |
183.00 | 1.00 | 1.3681 | 59.4 | 6.6 | 199.5 | 199.5 | 199.5 | 1.31 |
184.00 | 1.00 | 1.36809 | 63.6 | 4.2 | 199.4 | 199.5 | 199.5 | 0.83 |
185.00 | 1.00 | 1.36804 | 72.2 | 8.6 | 199.2 | 199.3 | 199.3 | 1.71 |
186.00 | 1.00 | 1.36811 | 79.9 | 7.7 | 199.5 | 199.3 | 199.3 | 1.54 |
187.00 | 1.00 | 1.36812 | 90.9 | 11.0 | 199.6 | 199.6 | 199.6 | 2.19 |
188.00 | 1.00 | 1.36809 | 100.2 | 9.3 | 199.4 | 199.5 | 199.5 | 1.86 |
189.00 | 1.00 | 1.36803 | 108.6 | 8.3 | 199.1 | 199.3 | 199.3 | 1.66 |
190.00 | 1.00 | 1.36803 | 117.0 | 8.4 | 199.1 | 199.1 | 199.1 | 1.68 |
191.00 | 1.00 | 1.36799 | 125.5 | 8.5 | 198.9 | 199.0 | 199.0 | 1.69 |
192.00 | 1.00 | 1.36763 | 133.8 | 8.3 | 196.8 | 197.8 | 197.8 | 1.65 |
193.00 | 1.00 | 1.36597 | 142.3 | 8.5 | 187.4 | 192.1 | 192.1 | 1.63 |
194.00 | 1.00 | 1.36174 | 153.2 | 10.9 | 163.3 | 175.3 | 175.3 | 1.91 |
195.00 | 1.00 | 1.35479 | 161.6 | 8.5 | 123.8 | 143.6 | 143.6 | 1.22 |
196.00 | 1.00 | 1.34658 | 170.0 | 8.3 | 77.1 | 100.4 | 100.4 | 0.84 |
197.00 | 1.00 | 1.3408 | 179.9 | 9.9 | 44.2 | 60.7 | 60.7 | 0.60 |
198.00 | 1.00 | 1.33723 | 186.3 | 6.5 | 23.9 | 34.1 | 34.1 | 0.22 |
199.00 | 1.00 | 1.33544 | 195.9 | 9.6 | 13.7 | 18.8 | 18.8 | 0.18 |
200.00 | 1.00 | 1.33457 | 204.0 | 8.1 | 8.8 | 11.3 | 11.3 | 0.09 |
201.00 | 1.00 | 1.33406 | 211.9 | 7.9 | 5.9 | 7.3 | 7.3 | 0.06 |
202.00 | 1.00 | 1.33376 | 221.4 | 9.6 | 4.2 | 5.0 | 5.0 | 0.05 |
203.00 | 1.00 | 1.33355 | 230.6 | 9.2 | 3.0 | 3.6 | 3.6 | 0.03 |
204.00 | 1.00 | 1.33348 | 236.5 | 5.9 | 2.6 | 2.8 | 2.8 | 0.02 |
205.00 | 1.00 | 1.33339 | 244.9 | 8.4 | 2.1 | 2.3 | 2.3 | 0.02 |
206.00 | 1.00 | 1.33331 | 252.8 | 7.9 | 1.6 | 1.8 | 1.8 | 0.01 |
207.00 | 1.00 | 1.33323 | 263.6 | 10.8 | 1.2 | 1.4 | 1.4 | 0.01 |
208.00 | 1.00 | 1.33316 | 271.5 | 7.9 | 0.8 | 1.0 | 1.0 | 0.01 |
209.00 | 1.00 | 1.33309 | 281.7 | 10.2 | 0.4 | 0.6 | 0.6 | 0.01 |
210.00 | 1.00 | 1.33307 | 289.7 | 8.0 | 0.3 | 0.3 | 0.3 | 0.00 |
211.00 | 1.00 | 1.333 | 297.7 | 8.0 | −0.1 | 0.1 | 0.1 | 0.00 |
212.00 | 1.00 | 1.33299 | 305.8 | 8.1 | −0.2 | −0.2 | −0.2 | 0.00 |
Total NaCl wash: 33 g |
-
- 1—Input of measurement data
- 2—Calculation of the first derivative
- 3—First derivative>0 or greater than a predefined value?
- 4—End of the washing operation
- 5—Error message
- 6—First derivative within a predefined range C?
- 7—Calculation of the average slope and variability (steps e-g)
- 8—Average slope and variability within the predefined ranges?
Claims (5)
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EP18167620.6 | 2018-04-16 | ||
EP18167620.6A EP3556447A1 (en) | 2018-04-16 | 2018-04-16 | Filtrate measurement-based monitoring of a filtration process |
PCT/EP2019/058886 WO2019201661A1 (en) | 2018-04-16 | 2019-04-09 | Process monitoring and control of filtration by means of filtrate measurements |
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US (1) | US11975276B2 (en) |
EP (2) | EP3556447A1 (en) |
JP (1) | JP7371005B2 (en) |
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EP4008420A1 (en) * | 2020-12-04 | 2022-06-08 | Bokela GmbH | Method and device for washing a filter cake on a filter medium |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US3815745A (en) * | 1971-01-27 | 1974-06-11 | N Mgeladze | Device for evaluating the quality of cake in intermittent filters |
EP0009527A1 (en) * | 1978-10-11 | 1980-04-16 | Myron Mantell | Process and apparatus for automatically controlling the washing of a filter cake |
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US4154677A (en) * | 1977-06-06 | 1979-05-15 | Myron Mantell | Automatic control of a filter bed wash process |
JP5072179B2 (en) * | 2004-12-24 | 2012-11-14 | 栗田工業株式会社 | Desalination cleaning method for waste |
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2018
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- 2019-04-09 AU AU2019256511A patent/AU2019256511A1/en not_active Abandoned
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3815745A (en) * | 1971-01-27 | 1974-06-11 | N Mgeladze | Device for evaluating the quality of cake in intermittent filters |
EP0009527A1 (en) * | 1978-10-11 | 1980-04-16 | Myron Mantell | Process and apparatus for automatically controlling the washing of a filter cake |
Non-Patent Citations (10)
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Kopra, R. et al. (2010), "Refractive index measurements for brown stock washing loss—mill investigations," Appita Journal, 63(2):131-136. |
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US20210146284A1 (en) | 2021-05-20 |
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EP3556447A1 (en) | 2019-10-23 |
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JP7371005B2 (en) | 2023-10-30 |
KR20210002479A (en) | 2021-01-08 |
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